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(4-Methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride → 4-(4-Methoxycarbonylbenzyl)-3-hydroxypyridine

HRID 2116490
ノート
印刷プレビュー

反応式

HRID 2116490 の反応式
Cl.[CH3:2][O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([CH:12]([C:14]2[CH:19]=[CH:18][N:17]=[CH:16][C:15]=2[OH:20])O)=[CH:8][CH:7]=1)=[O:5]>[Pd].CO>[CH3:2][O:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]([CH2:12][C:14]2[CH:19]=[CH:18][N:17]=[CH:16][C:15]=2[OH:20])=[CH:10][CH:11]=1)=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 23103650(4-Methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride

生成物 1

HCID 231036354-(4-Methoxycarbonylbenzyl)-3-hydroxypyridine収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Next, a mixture of (4-methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride (1.87 g, 5.50 mmol), methanol (50 ml) and 10% palladium/carbon (0.94 g) was stirred under a hydrogen atmosphere at room temperature for 3 days. After filtration to remove the insoluble materials, the filtrate was concentrated under reduced pressure and the resulting residue was poured into saturated aqueous NaHCO3 and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting crystal was recrystallized from diethyl ether to give the titled compound (1.27 g, 95%).

後処理

  1. filtrationAfter filtration
  2. customto remove the insoluble materials
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionthe resulting residue was poured into saturated aqueous NaHCO3
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting crystal was recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-2b7bf570d3154c73af2b6f98d5817ece
出典データセット
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07439232B2

反応ノート

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